CN1063309A - The solvent extraction method concentration process of gibberellin fermented filtrate - Google Patents
The solvent extraction method concentration process of gibberellin fermented filtrate Download PDFInfo
- Publication number
- CN1063309A CN1063309A CN 91100074 CN91100074A CN1063309A CN 1063309 A CN1063309 A CN 1063309A CN 91100074 CN91100074 CN 91100074 CN 91100074 A CN91100074 A CN 91100074A CN 1063309 A CN1063309 A CN 1063309A
- Authority
- CN
- China
- Prior art keywords
- extraction
- gibberellins
- organic phase
- volume ratio
- fermented filtrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention is a kind of solvent extraction method concentration process of gibberellin fermented filtrate, belongs to the Plant hormones regulators,gibberellins production field.Gibberellin fermented filtrate is transferred to pH=2.0～3.0, organic phase (volume fraction of extraction agent is 30～60%) with organophosphorus (phosphine) class and/or amine extractant and sulfonated kerosene diluent composition is mixed the extraction of carrying out Plant hormones regulators,gibberellins with aqueous phase liquid, the volume ratio of control organic phase and water is 1: 2～5, then uses saturated NaHCO
3Solution is stripped, and the volume ratio of control strip aqueous and load organic phases is 1: 3～5, and the extraction and the operation of stripping are all carried out at normal temperatures.This process recovery ratio height, low, the non-environmental-pollution of energy consumption.
Description
The present invention is a kind of solvent extraction method concentration process of gibberellin fermented filtrate, belongs to the Plant hormones regulators,gibberellins production field.
Plant hormones regulators,gibberellins (Gibberellins, domestic being commonly called as " 920 ") is a kind of efficient plant growth element and conditioning agent.It is mainly used in volume increase and the precocity of hybrid rice, cotton, wheat, fruit and vegetables etc.The healing of accelerating the surface of a wound to the cultivation of flowers with on clinical medicine also has effect preferably.
Plant hormones regulators,gibberellins is to be a class homologue of basic framework with gibberic acid alkane, isolates more than 70 kind of compound at present altogether from microorganism and plant, wherein with Plant hormones regulators,gibberellins A
3(GA
3) active maximum.GA
3Molecular formula be C
19H
22O
6, structural formula is:
Molecular weight is 346.
The production process of Plant hormones regulators,gibberellins is to be microbial process, and it produces by fermentation, and GA content is about 1000～1500u/ml in the gained fermented liquid.The key step of its follow-up extraction, purge process is as follows: at first fermented liquid is given processing, promptly be acidified with acid to PH=2.0～2.5, at this moment will there be most of albumen to settle out, carry out the filtration of acidizing fluid then with filter press, at this moment mycelium can be filtered together with the albumen that settles out and must be crossed cleaner liquid; Using Na below 15 ℃
2CO
3Readjustment filtrate acidity is to PH=4.5～5.0; Send acidizing fluid to go to concentrate; Existing concentration method mainly is a method of evaporation, and evaporation equipment has thin-film evaporator and still formula vaporizer etc.; The control vaporization temperature is lower than 50 ℃ under the 0.08MPa vacuum condition, with filtrate concentrate about 10～15 times and concentrated solution; Be refrigerated to and use vitriol oil acidifying concentrated solution to PH=2.0～2.5 below 15 ℃ again, the back is carried out cross current solvent extraction twice with ethyl acetate, and extracting operation is many to carry out in stirring tank, and carries out the centrifugal phase-splitting of mixed solution with tubular-bowl centrifuge; Come together to such an extent that liquid is 0.08MPa in vacuum tightness in still formula vaporizer, carries out evaporation concentration below 35 ℃ and get the Plant hormones regulators,gibberellins crystallization to the gained ethyl ester; The crystal that must wet after filtration, mother liquor deallocation system " 920 " emulsion; Wet crystal by comparing 1: 1 washed twice, is sent to oven dry after washing once with ethyl ester again with the aqueous solution of PH=4.5～5.0, and controlled temperature is 45 ± 5 ℃, and the time is 3～4 hours; Promptly carry out packing behind the crystal palpus crushing screening (sieve aperture is 40 orders) of drying and get finished product.
The clear 55-120794 of Japanese Patent etc. has reported with the method for charcoal absorption with purifying and concentrated Plant hormones regulators,gibberellins; Get 10 liters of fermented liquids, pH value to 2 with the hydrochloric acid flavouring liquid, the adding gac soaks and stirs one hour, filtration, gained gac filter cake is used the 5 liters of immersions of strong aqua that contain 1% methyl alcohol and is concentrated to 0.5 liter, transfer the pH value to 2 of concentrated solution again with hydrochloric acid, with 2 liters of ethyl acetate extractions, extraction liquid is concentrated to 0.5 liter, use 2 liter 1% NaHCO then
3The aqueous solution is stripped; Transfer PH to 2 again,, and will come together to such an extent that liquid is concentrated to 0.5 liter with 5 liters of ethyl acetate extractions; Add Na
2SO
4Dehydration promptly gets the Plant hormones regulators,gibberellins crystallization through further concentrating.Except charcoal absorption, specifically do not provide concentration method in the literary composition, estimate it mainly also is the method for evaporation.
Its loss mainly is at the evaporation concentration treatment step in aforesaid Plant hormones regulators,gibberellins production process, and up to 10～15%, this is because the sensitive characteristic of Plant hormones regulators,gibberellins causes.In addition, evaporation concentration also has following shortcoming:
(1) because of transforming, the negative pressure of having relatively high expectations and coal one vapour make energy consumption higher during evaporation concentration;
(2) in evaporating concentration process, Plant hormones regulators,gibberellins there is not purification effect, and the general thickness comparatively of the feed liquid after concentrating, the solid settlement thing is arranged, follow-up ethyl acetate extraction process there is detrimentally affect.
The present invention studies at this weak link in the Plant hormones regulators,gibberellins production process just, has promptly adopted solvent extraction circuit to replace evaporation to carry out concentrating of gibberellin fermented filtrate.
The present invention is the solvent extraction method concentration process of gibberellin fermented filtrate, gibberellin fermented filtrate is transferred to PH=2.0～3.0, mix the extraction of carrying out Plant hormones regulators,gibberellins with aqueous phase liquid with the organic phase (volume fraction of extraction agent is 30～60%) that extraction agent and sulfonated kerosene diluent are formed, the volume ratio of control organic phase and water is 1: 2～5, then uses saturated NaHCO
3Solution is stripped, and the volume ratio of control strip aqueous and load organic phases is 1: 3～5, and the extraction and the operation of stripping are all carried out at normal temperatures.Said extraction agent can be organophosphorus (phosphine) class, also can be amine, also can be the mixture of organophosphorus (phosphine) class and amine, adds n-Octanol under the amine extractant situation, and said organophosphorus (phosphine) class is meant down a kind of in the array structure:
Said amine is meant down a kind of in the array structure:
R
3N （R＝CnH
2n+1，n＝8～10）
R
3N
+CH
3Cl
-（R＝CnH
2n+1，n＝8～11）
（R≥C
1，R′≥C
1）
Describe the present invention below.The basic procedure of this technology is as shown below:
At first add the vitriol oil and to gibberellin fermented filtrate, regulate pH value to 2.0～3.0, send into multi-stage solvent extraction device and the organic phase (mixed solution of Phosphorus [phosphine class], amine extractant and sulfonated kerosene for preparing then, under the amine extractant situation, added alcohols) contact, extraction is carried out continuously with reflux type at ambient temperature, and the volume ratio of control organic phase and water is 1: 2～5, effusive two-phase be respectively come together organic phase (or being referred to as load organic phases) and aqueous extraction residue.
In order to remove the organic phase that in aqueous residue, may carry secretly effectively, before discharging, at first deliver to the oily-water seperating equipment oil removing, discharging after neutralizing again.
Come together to such an extent that organic phase goes to pick into reextraction device and strip liquor (saturated NaHCO
3Solution) contact to realize the reextraction of Plant hormones regulators,gibberellins, stripping also is to carry out continuously with reflux type at ambient temperature, the control strip aqueous with come together to such an extent that the volume ratio of organic phase is 1: 3～5, at this moment effusive two-phase is respectively dense back extraction concentrated solution and the organic phase after Plant hormones regulators,gibberellins is removed in back extraction of having adopted Plant hormones regulators,gibberellins.The back extraction concentrated solution enters next treatment step (ethyl acetate extraction), organic phase round-robin after simple process after the back extraction after transferring PH.
Used thinner is a sulfonated kerosene, and it consists of normal alkane content: 98.3%(wt), and aromaticity content＜0.001%(wt); Its rerum natura is: proportion (20 ℃) 0.75g/cm
3, boiling point 198-241 ℃, 70 ℃ of flash-points, viscosity (20 ℃) 1.9345mPa.s.
Adopt solvent extraction to carry out spissated method and can obtain following techno-economic effect:
(1) makes gibberellin fermented filtrate concentrate 10～20 times, reach the concentration technology requirement.
(2) concentrated solution is transparent, does not have precipitation, is convenient to subsequent disposal.
(3), thereby improve the quality of products because used extraction agent can make Plant hormones regulators,gibberellins obtain to a certain degree purifying for the extraction selectivity of Plant hormones regulators,gibberellins by extracting operation.
(4) used extraction agent is water-soluble low, can round-robin, prevented pollution simultaneously to environment.
(5) have remarkable economic efficiency, increasing benefit in year for a factory that produces 10 tons of Plant hormones regulators,gibberellins per year can reach more than 2,000,000 yuan, this be because:
ⅰ) the raising of Plant hormones regulators,gibberellins yield; Because extraction, the operation of stripping are all carried out at normal temperatures, do not have the heat loss of Plant hormones regulators,gibberellins, thereby have reduced the loss of Plant hormones regulators,gibberellins in concentration process significantly, its rate of loss is reduced to below 5%, and promptly its rate of recovery concentrates and improves more than 10% than evaporation.
ⅱ) again owing to the less power consumption of normal-temperature operation and extracting operation, its energy consumption has reduction significantly than method of evaporating.
Claims (3)
1, a kind of solvent extraction method concentration process of gibberellin fermented filtrate, it is characterized in that gibberellin fermented filtrate is transferred to PH=2.0～3.0, mix the extraction of carrying out Plant hormones regulators,gibberellins with aqueous phase liquid with the organic phase (volume fraction of extraction agent is 30～60%) that extraction agent and sulfonated kerosene diluent are formed, the volume ratio of control organic phase and water is 1: 2～5, then uses saturated NaHCO
3Solution is stripped, and the volume ratio of control strip aqueous and load organic phases is 1: 3～5, and the extraction and the operation of stripping are all carried out at normal temperatures, said extraction agent under a kind of organophosphorus (phosphine) in the array structure:
2, a kind of solvent extraction method concentration process of gibberellin fermented filtrate, it is characterized in that gibberellin fermented filtrate is transferred to PH=2.0～3.0, mix the extraction of carrying out Plant hormones regulators,gibberellins with aqueous phase liquid with the organic phase (volume fraction of extraction agent is 30%～60%) that extraction agent and sulfonated kerosene diluent are formed, the volume ratio of control organic phase and water is 1: 2～5, then uses saturated NaHCO
3Solution is stripped, and the volume ratio of control strip aqueous and load organic phases is 1: 3～5, and the extraction and the operation of stripping are all carried out at normal temperatures, said extraction agent under a kind of amine in the array structure, and added n-Octanol,
R
3N （R＝CnH
2n+1，n＝8～10）
R
3N
+CH
3Cl
-（R＝CnH
2n+1，n＝8～11）
3, a kind of solvent extraction method concentration process of gibberellin fermented filtrate, it is characterized in that gibberellin fermented filtrate is transferred to PH=2.0～3.0, mix the extraction of carrying out Plant hormones regulators,gibberellins with aqueous phase liquid with the organic phase (volume fraction of extraction agent is 30～60%) that extraction agent and sulfonated kerosene diluent are formed, the volume ratio of control organic phase and water is 1: 2～5, then uses saturated NaHCO
3Solution is stripped, and the volume ratio of control strip aqueous and load organic phases is 1: 3～5, and the extraction and the operation of stripping are all carried out at normal temperatures, said extraction agent under a kind of organophosphorus (phosphine) in the array structure and a kind of mixture of amine:
Organophosphorus (phosphine):
Amine:
R
3N （R＝CnH
2n+1，n＝8～10）
R
3N
+CH
3Cl
-（R＝CnH
2n+1，n＝8～11）
（R≥C
1，R′≥C
1）
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91100074 CN1033520C (en) | 1991-01-11 | 1991-01-11 | Solvent extraction method concentration process of gibberellin fermented filtrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91100074 CN1033520C (en) | 1991-01-11 | 1991-01-11 | Solvent extraction method concentration process of gibberellin fermented filtrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1063309A true CN1063309A (en) | 1992-08-05 |
| CN1033520C CN1033520C (en) | 1996-12-11 |
Family
ID=4904434
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91100074 Expired - Fee Related CN1033520C (en) | 1991-01-11 | 1991-01-11 | Solvent extraction method concentration process of gibberellin fermented filtrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1033520C (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045959C (en) * | 1995-03-16 | 1999-10-27 | 北京农业大学 | Method for stage extraction gibberellin A4 and A7 from gibberellin mixture |
| CN102127581A (en) * | 2010-12-22 | 2011-07-20 | 江西核工业瑞丰生化有限责任公司 | Method for improving extraction yield of gibberellin |
| CN102942547A (en) * | 2012-11-16 | 2013-02-27 | 南京工业大学 | GA4And/or GA7Separation and purification method of |
| CN104672190A (en) * | 2014-12-12 | 2015-06-03 | 江西新瑞丰生化有限公司 | Method for recrystallizing gibberellin mother liquor |
| CN105000973A (en) * | 2015-06-30 | 2015-10-28 | 芜湖福民生物药业有限公司 | Gibberellin preparation, and preparation method and applications thereof |
| CN107988305A (en) * | 2018-01-18 | 2018-05-04 | 四川龙蟒福生科技有限责任公司 | The preparation method of gibberellic acid |
-
1991
- 1991-01-11 CN CN 91100074 patent/CN1033520C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045959C (en) * | 1995-03-16 | 1999-10-27 | 北京农业大学 | Method for stage extraction gibberellin A4 and A7 from gibberellin mixture |
| CN102127581A (en) * | 2010-12-22 | 2011-07-20 | 江西核工业瑞丰生化有限责任公司 | Method for improving extraction yield of gibberellin |
| CN102127581B (en) * | 2010-12-22 | 2014-11-05 | 江西新瑞丰生化有限公司 | Method for improving extraction yield of gibberellin |
| CN102942547A (en) * | 2012-11-16 | 2013-02-27 | 南京工业大学 | GA4And/or GA7Separation and purification method of |
| CN102942547B (en) * | 2012-11-16 | 2016-02-10 | 南京工业大学 | GA4And/or GA7Separation and purification method of |
| CN104672190A (en) * | 2014-12-12 | 2015-06-03 | 江西新瑞丰生化有限公司 | Method for recrystallizing gibberellin mother liquor |
| CN104672190B (en) * | 2014-12-12 | 2017-04-19 | 江西新瑞丰生化有限公司 | Method for recrystallizing gibberellin mother liquor |
| CN105000973A (en) * | 2015-06-30 | 2015-10-28 | 芜湖福民生物药业有限公司 | Gibberellin preparation, and preparation method and applications thereof |
| CN107988305A (en) * | 2018-01-18 | 2018-05-04 | 四川龙蟒福生科技有限责任公司 | The preparation method of gibberellic acid |
| CN107988305B (en) * | 2018-01-18 | 2021-07-02 | 四川龙蟒福生科技有限责任公司 | Preparation method of gibberellic acid |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1033520C (en) | 1996-12-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US6478965B1 (en) | Recovery of fermentation salts from dilute aqueous solutions | |
| JPH09500649A (en) | Organic acid recovery method | |
| WO2012051774A1 (en) | Process for salting out and extracting organic acid from fermentation broth | |
| CN1033520C (en) | Solvent extraction method concentration process of gibberellin fermented filtrate | |
| CN107337593B (en) | Preparation method of coenzyme Q10 pure product | |
| CN114436816B (en) | Method for efficiently extracting shikimic acid by ion exchange technology | |
| CN1290812C (en) | Method for extracting xylitol from xylitol mother liquor | |
| JPH01271496A (en) | Extracting method of sugarcane lipid component (cane wax) | |
| CN102206241B (en) | Technological process for extracting ergosterol with high purity and feed protein from penicillin waste residue | |
| CN114853593A (en) | Method for extracting high-purity nervonic acid from acer truncatum buge oil | |
| CN113861262A (en) | Tomatidine extraction and concentration process | |
| CN1021443C (en) | Method for extracting lincomycin by solvent | |
| CN1300131C (en) | Separation method for purifying gibberellin GA3 | |
| CN1047773C (en) | Method for preparation of natural carotene | |
| CN1055738A (en) | Gibberellin extraction process | |
| CN1162440C (en) | Process for preparation of 1,6-anhydro-beta-D-pyranoglucose from self-pyrolyzed oil | |
| CN1196340A (en) | High-efficiency boron-magnesium fertilizer and producing method | |
| CN1060217C (en) | Extracting process of carotene from trispore bruce mould | |
| CN1348992A (en) | Continuous single-tank fermentation process of bacillus in membrane coupled clear liquid for producing levolactic acid | |
| CN106673996A (en) | Method for purifying long-chain dicarboxylic acid | |
| US3385764A (en) | Process for preparation of fusafungine | |
| CN116751110A (en) | Method for extracting inositol from inositol mother liquor | |
| CN115772198A (en) | Novel method for desugaring abamectin | |
| RU2051594C1 (en) | Method of preparing pectin from plant raw | |
| CN116271973A (en) | Method and device for extracting fermentation product |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |